CN113926487A - Fullerol/palladium nano composite photocatalyst and preparation method and application thereof - Google Patents

Fullerol/palladium nano composite photocatalyst and preparation method and application thereof Download PDF

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CN113926487A
CN113926487A CN202111075752.0A CN202111075752A CN113926487A CN 113926487 A CN113926487 A CN 113926487A CN 202111075752 A CN202111075752 A CN 202111075752A CN 113926487 A CN113926487 A CN 113926487A
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fullerol
mixed solution
palladium
composite photocatalyst
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高鹏
吴文博
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Hangzhou Normal University
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    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/0201—Oxygen-containing compounds
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    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
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    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract

The invention relates to the field of photocatalysts and discloses a fullerol/palladium nano composite photocatalyst as well as a preparation method and application thereof, wherein the chemical formula of the fullerol in the scheme is C60(OH)44.8H2O, the palladium nanoparticles have an average particle diameter of 3 to 4nm and are used for CO2And (4) carrying out photocatalytic reduction. The invention can effectively delay and block the recombination of photo-generated electron-hole pairs, thereby achieving better photocatalysis effect; the prepared fullerol and palladium nano composite photocatalyst has the characteristics of uniform size, good crystallinity, high catalytic efficiency and high catalytic speed; the obtained richThe average particle size of palladium metal particles in the methanol and palladium nano composite photocatalyst is 3-4nm, and the fullerene alcohol is easy to capture electrons; green and environment-friendly, and can be recycled.

Description

Fullerol/palladium nano composite photocatalyst and preparation method and application thereof
Technical Field
The invention relates to the field of photocatalysts, in particular to a fullerol/palladium nano composite photocatalyst and a preparation method and application thereof.
Background
Fullerene is a carbon cluster-structured molecule C60 consisting of 60 carbons. Comprising twenty six-membered rings and twelve five-membered rings. Unlike sp2 hybridization in graphite, which is in the same plane, the conjugated pi bond in fullerene is non-planar, so that the ring current is small and the aromaticity is poor, showing the property of unsaturated double bond. That is, although the carbon atoms in the fullerene molecule are all hyperconjugated, the fullerene is not aromatic as a whole. Due to the presence of twelve five-membered rings, fullerenes require an additional 12 electrons to form the most stable closed shell system. Thus, fullerenes readily trap electrons and are good hosts for metal atoms. Both electron-phonon and electron-electron interactions of fullerenes are large on the energy scale of the expected narrow bandwidth, with strong electron-electron interactions approaching the mott-hubbard type metal-insulator transitions. The fullerene alcohol is a compound in which a hydroxyl group is introduced into fullerene in order to improve the water solubility of fullerene. But the fullerol has water solubility only when the number of hydroxyl groups reaches a certain value. Generally, the hydroxyl number reaches more than 20 to have better water solubility, and the chemical property is similar to that of fullerene.
The electron negativity of the fullerene is reduced due to the introduced electron donating group-OH, so that the fullerene not only preserves the addition activity of the fullerene, but also reduces the toxicity to organisms, and greatly improves the biocompatibility. Therefore, the fullerol and the composite material thereof have certain application values in the aspects of oxidation resistance, drug carriers, high polymer materials, solar cells, proton conductors and the like. Among the numerous promoters, the most significant improvement effects on photocatalytic performance are Pt, Pd, Au, and the like. Pd is widely applied to photolysis of water to generate hydrogen and CO by virtue of the advantages of excellent characteristics and physicochemical properties of Pd and remarkable improvement on the reaction activity of a main catalyst and the like2The field of reduction. However, the existing Pd catalyst has poor catalytic efficiency and is used for CO2The reaction rate in the reduction field is also relatively slow.
Publication No. CN113173575A discloses a copper nanoparticle/fullerol nanocomposite material, and a preparation method and application thereof, belonging to the technical field of nanomaterials. According to the preparation method, fullerene is used as a matrix, the fullerene is subjected to hydroxylation modification to obtain fullerol, copper ions in copper chloride are reduced into copper nanoparticles through laser photoreduction, and the copper nanoparticles are stably loaded on the surface of the fullerol, so that the copper nanoparticle/fullerol composite material is prepared. But it is not applied to CO2The field of reduction.
Disclosure of Invention
In order to solve the technical problems, the invention provides a fullerol/palladium nano composite photocatalyst and a preparation method and application thereof. According to the invention, the prepared fullerene alcohol and palladium nano composite photocatalyst is uniform in size and good in crystallinity by compounding the fullerene alcohol and the palladium, and has the characteristics of high catalytic efficiency and high catalytic speed; the average particle size of palladium metal particles in the prepared fullerol and palladium nano composite photocatalyst is 3-4nm, and the fullerol is easy to capture electrons.
The specific technical scheme of the invention is as follows: a fullerol/palladium nano composite photocatalyst, the fullerol chemical formula is C60(OH)44.8H2And O, wherein the average particle size of the palladium nano-particles is 3-4 nm.
According to the invention, the fullerol and palladium nano composite photocatalyst with uniform size and good crystallinity is prepared by compounding the fullerol and the palladium, the average particle size of palladium metal particles is 3-4nm, stronger interaction exists between the fullerol and the palladium nano particles, electron transfer exists, the catalyst has the characteristics of high catalytic efficiency and high catalytic speed, the palladium nano particles are uniformly loaded on the fullerol, and the prepared fullerol and palladium nano composite photocatalyst has the advantages that the fullerol is easy to capture electrons and can be an excellent host of metal atoms.
The invention also provides a preparation method of the fullerol/palladium nano composite photocatalyst, which comprises the following steps:
(1) according to a molar ratio of 1: 350-390 adding C60 into solvent A to obtain mixed solution A, and then mixing the mixed solution A with H2O2Mixing to obtain a mixed solution B, wherein C60 and H in the mixed solution B2O2In a molar ratio of 1: 320-370.
(2) Mixing the mixed solution B with TBAH, heating for reaction to obtain Fullerol C60(OH)44.8H2O, a crude product;
(3) mixing C60(OH) obtained in step (2)44.8H2Treating the crude O product with mixed solution of isopropanol, ethyl acetate and n-hexane to obtain light yellow precipitate, cleaning, and drying to obtain fullerol C60(OH)44.8H2O；
(4) And dispersing the fullerol and sodium tetrachloropalladate into a solvent B, reacting for 2-3h under the illumination condition, treating with a mixed solution of isopropanol, ethyl acetate and n-hexane, and cleaning and drying to obtain the fullerol/palladium nano composite photocatalyst.
TBAH is used as a phase transfer catalyst, so that the conversion rate and the yield of the product can be improved. Promoting fullerol C60(OH) by mixed solution of isopropanol, ethyl acetate and n-hexane44.8H2And (4) recrystallizing O.
Preferably, in step (1), the solvent A is 1, 2, 4-trimethylbenzene.
The fullerene is more soluble in 1, 2, 4-trimethylbenzene, thereby promoting a more complete reaction.
Preferably, in the step (2), the heating method is a water bath or an oil bath, the temperature is 60-80 ℃, and the reaction time is 15-17 h.
Preferably, in the step (3), the cleaning method is alternately cleaning with deionized water and methanol, and the drying condition is vacuum drying at room temperature for 8-10 hours.
Preferably, in the step (3), the mass ratio of isopropanol, ethyl acetate and n-hexane in the mixed solution is 5: 3.8-4.2: 4.8-5.2.
When the concentration ratio of the mixed solution of isopropanol, ethyl acetate and n-hexane is out of the range, the fullerol C60(OH)44.8H2The O recrystallization effect becomes poor.
Preferably, in the step (4), the fullerol is mixed with Na2PdCl41: 6.5-7.5; the solvent B is a methanol solution with the concentration of 2.0-2.5mol/L, and the concentration of the fullerol in the solvent B is 1.5-2.0 g/L.
Methanol acts as a reducing agent to participate in the reaction.
Preferably, in step (4), the reaction is carried out under the illumination condition: stirring under visible light at room temperature for 2-3 h.
The reaction time has great influence on the size and the loading capacity of Pd, and when the reaction time is too long, the loaded metal palladium particles are too large, the reaction time is too short, and the loading effect is not ideal.
Preferably, in the step (4), the mass ratio of isopropanol, ethyl acetate and n-hexane in the mixed solution is 5: 3.8-4.2: 4.8-5.2.
The invention also discloses the application of the fullerol/palladium nano composite photocatalyst in CO2And (4) carrying out photocatalytic reduction.
Compared with the prior art, the invention has the beneficial effects that:
(1) can effectively delay and block the recombination of the photoproduction electron-hole pair, thereby achieving better photocatalysis effect.
(2) The prepared fullerol and palladium nano composite photocatalyst has the characteristics of uniform size, good crystallinity, high catalytic efficiency and high catalytic speed; the average particle size of palladium metal particles in the prepared fullerol and palladium nano composite photocatalyst is 3-4nm, and the fullerol is easy to capture electrons;
(3) green and environment-friendly, and can be recycled.
Drawings
FIG. 1 is an XRD diagram of a fullerol/palladium nano-composite photocatalyst prepared in example 1 of the present invention.
FIG. 2 is a TEM image of the fullerol/palladium nanocomposite photocatalyst prepared in example 1 of the present invention.
FIG. 3 is a FT-IR diagram of a fullerol/palladium nanocomposite photocatalyst prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. The devices, reagents and methods referred to in the present invention are those known in the art unless otherwise specified.
Example 1
(1) Preparation of Fullerol (C60(OH)44.8H2O): 0.100g C60 was added to the beaker, 7mL of 1, 2, 4-trimethylbenzene solution was added to disperse C60, and 4.6mL of 30% H was added2O2C60 and 30% H2O2The molar ratio of (1: 320), the mixture is completely dissolved after being magnetically stirred for 30 minutes in an oil bath at the temperature of 60 ℃, then the TBAH is added in an amount of 400 mu L, and the mixture is magnetically stirred for 16 hours; separating a light yellow aqueous solution from the obtained solution, wherein the mass ratio of the light yellow aqueous solution to the light yellow aqueous solution is 5: 4: 5 isopropanol ethyl acetate:and mixing the n-hexane mixed solution to obtain a milky white precipitate. The precipitate was washed with deionized water 2 times, with methanol 2 times, and then dried under vacuum at room temperature for 10 hours.
(2) Preparing a fullerol/palladium nano composite photocatalyst: 0.0161g of fullerol was added to a clean beaker, 50mL of water was added, and 0.0208g of Na was added2PdCl45mL of methanol is stirred and dissolved, the concentration of the methanol solution of the fullerol is 1.82g/L, and the fullerol is mixed with Na2PdCl41: 7. the reaction was stirred at room temperature under visible light for 2 h. And (3) mixing the obtained solution with a solvent in a mass ratio of 5: 4: 5 isopropanol ethyl acetate: and mixing the n-hexane mixed solution to obtain dark brown precipitate, washing with water for 2 times, and drying in vacuum at room temperature for 10 hours to obtain the fullerol/palladium nano composite photocatalyst. The diameter of the prepared Pd nano-particles is 4 nm.
Example 2
The difference from example 1 is C60 and 30% H2O2Is 1: 340.
Example 3
The difference from example 1 is C60 and 30% H2O2In a molar ratio of 1: 350.
Example 4
The difference from example 1 is C60 and 30% H2O2In a molar ratio of 1: 370.
Example 5
The difference from example 1 is that the reaction was stirred under visible light conditions for 2 h.
Example 6
The difference from example 1 is that the reaction was stirred under visible light conditions for 3 h.
Example 7
The difference from example 1 is that fullerol is mixed with Na2PdCl41: 6.5.
example 8
The difference from example 1 is that fullerol is mixed with Na2PdCl41: 7.5.
comparative example 1
The difference from example 1 is that no Pd was supported.
Comparative example 2
The difference from example 1 is C60 and 30% H2O2Is 1: 280.
Comparative example 3
The difference from example 1 is C60 and 30% H2O2In a molar ratio of 1: 400.
Comparative example 4
The difference from example 1 is that fullerol is mixed with Na2PdCl41: 8.
comparative example 5
The difference from example 1 is that fullerol is mixed with Na2PdCl41: 6.
comparative example 6
The difference from example 1 is that the reaction was stirred under visible light conditions for 1 h.
Comparative example 7
The difference from example 1 is that the reaction was stirred under visible light conditions for 4 h.
Performance testing
The fullerol/palladium nano composite photocatalyst prepared in the examples 1 to 7 and the comparative examples 1 to 7 is used for catalyzing CO photocatalysis2Reduction reaction, catalyst dosage 3mg, CO and CH under visible light4The trend of the yield over time is shown in the table below, which shows that the catalyst has excellent catalytic performance.
Results of Performance testing
The catalysts prepared in examples 1 to 7 and comparative examples 1 to 7 were used for photocatalytic CO2Reduction reaction, catalyst dosage 3mg, CO and CH under visible light4The trend of the yield over time is shown in the table below, which shows that the catalyst has excellent catalytic performance.
1h 2h 3h 4h 5h
Example 1 12.5μmol/g 13.8μmol/g 14.6μmol/g 15.9μmol/g 17.0μmol/g
Example 2 12.6μmol/g 14.1μmol/g 15.6μmol/g 16.8μmol/g 18.6μmol/g
Example 3 13μmol/g 14.2μmol/g 15.6μmol/g 17.2μmol/g 19.1μmol/g
Example 4 12.2μmol/g 13.6μmol/g 14.8μmol/g 16μmol/g 17.8μmol/g
Example 5 13.6μmol/g 14.4μmol/g 15.8μmol/g 17.6μmol/g 18.9μmol/g
Example 6 12.8μmol/g 13.8μmol/g 14.9μmol/g 15.6μmol/g 16.8μmol/g
Example 7 13μmol/g 14.6μmol/g 15.5μmol/g 16.2μmol/g 17.4μmol/g
Comparative example 1 0.5μmol/g 0.7μmol/g 0.9μmol/g 1.2μmol/g 1.3μmol/g
Comparative example 2 6.6μmol/g 7.8μmol/g 9.0μmol/g 9.8μmol/g 10.2μmol/g
Comparative example 3 4.3μmol/g 5μmol/g 5.9μmol/g 6.7μmol/g 8.1μmol/g
Comparative example 4 4.4μmol/g 5.2μmol/g 6μmol/g 7.2μmol/g 8.6μmol/g
Comparative example 5 7.4μmol/g 8.1μmol/g 9mol/g 10.9μmol/g 11.8μmol/g
Comparative example 6 7.2μmol/g 9.6μmol/g 10.8μmol/g 11.9μmol/g 12.8μmol/g
Comparative example 7 8.2μmol/g 9.9μmol/g 11μmol/g 12.6μmol/g 13.9μmol/g
As can be seen from the results of examples 1 to 7 and comparative examples 1 to 7, with respect to C60 and 30% H2O2In an optimum ratio when H is added2O2In excess, excessive side reactions may be introduced, leading to fullerene or fullerol oxidation; when H is present2O2If the fullerene reaction is too low, the fullerene reaction is incomplete, so that the comparative examples 2 to 3 have poor effects, so that the problem of excessive amount of any one of the two is solved, the subsequent treatment and purification of the sample are not facilitated, and the performance of the sample is greatly reduced due to excessive impurities in the sample. If the sodium tetrachloropalladate is too much, the loading capacity on the fullerol is too much, the surface can form agglomeration to be unfavorable for absorbing and desorbing reactants, so that the performance is reduced, and if the sodium tetrachloropalladate is too little, the reaction speed is too slow, the performance is reduced, so that the effect of the comparative examples 4-5 is poorer. The reaction time determines the size and the load uniformity of the palladium metal particles, the metal palladium particles are larger after more than 3 hours, and too much load on the fullerol is caused, the surface agglomeration is formed to be unfavorable for absorbing and desorbing reactants, so that the performance is reduced, the short time causes the insufficient load on the fullerol, the reaction is too slow, so that the performance is reduced, and the comparative examples 6-7 have poor effects. Comparative example 1 does not support a palladium atom and is inferior to the other examples and comparative examples in performance.
And (3) performance characterization:
XRD (X-ray diffraction) testing is carried out on the fullerol/palladium nano-composite photocatalyst prepared in the embodiment 1 of the invention, the morphology of the fullerol/palladium nano-composite photocatalyst is observed by adopting a TEM (transmission electron microscope), and the structure of the fullerol/palladium nano-composite photocatalyst is tested by adopting an FT-IR (FT-IR) diagram.
And (3) performance characterization results:
1. as can be seen from fig. 1, the fullerol/palladium nano composite photocatalyst prepared by the embodiment 1 of the invention has good crystallinity, no other impurities are generated, and the purity is high;
2. as can be seen from fig. 2, the fullerol/palladium nano composite photocatalyst prepared by the embodiment 1 of the invention has regular morphology and is well compounded with Pd metal particles;
3. as is clear from fig. 3, in the fullerene alcohol/palladium nanocomposite photocatalyst produced in example 1 of the present invention, the structure of the fullerene alcohol was not significantly changed, and the original structure was maintained.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.

Claims (10)

1. A fullerol/palladium nano composite photocatalyst is characterized in that the fullerol has a chemical formula of C60(OH)44.8H2And O, wherein the average particle size of the palladium nano-particles is 3-4 nm.
2. A method for preparing a fullerol/palladium nano-composite photocatalyst as claimed in claim 1, which comprises the following steps:
(1) according to a molar ratio of 1: 350-390 reaction of C60Adding into solvent A to obtain mixed solution A, and mixing the mixed solution A with H2O2Mixing to obtain a mixed solution B, wherein C in the mixed solution B60And H2O2The molar ratio of (1: 320) -;
(2) mixing the mixed solution B with TBAH, heating for reaction to obtain Fullerol C60(OH)44.8H2O, a crude product;
(3) mixing C60(OH) obtained in step (2)44.8H2Treating the crude O product with mixed solution of isopropanol, ethyl acetate and n-hexane to obtain light yellow precipitate, cleaning, and drying to obtain fullerol C60(OH)44.8H2O；
(4) And dispersing the fullerol and sodium tetrachloropalladate into a solvent B, reacting under the illumination condition, treating by using a mixed solution of isopropanol, ethyl acetate and n-hexane, and cleaning and drying to obtain the fullerol/palladium nano composite photocatalyst.
3. The method according to claim 2, wherein in the step (1), the solvent A is 1, 2, 4-trimethylbenzene.
4. The method according to claim 2, wherein in the step (2), the heating method is a water bath or an oil bath, the temperature is 60-80 ℃, and the reaction time is 15-17 h.
5. The method according to claim 2, wherein in the step (3), the washing is performed by alternately washing with deionized water and methanol, and the drying is performed under vacuum at room temperature for 8 to 10 hours.
6. The preparation method according to claim 2, wherein in the step (3), the mass ratio of isopropanol, ethyl acetate and n-hexane in the mixed solution is 5: 3.8-4.2: 4.8-5.2.
7. The method according to claim 2, wherein in the step (4), the fullerol is mixed with Na2PdCl41: 6.5-7.5; the solvent B is a methanol solution with the concentration of 2.0-2.5mol/L, and the concentration of the fullerol in the solvent B is 1.5-2.0 g/L.
8. The method according to claim 2, wherein in the step (4), the reaction is carried out under light: stirring under visible light at room temperature for 2-3 h.
9. The preparation method according to claim 2, wherein in the step (4), the mass ratio of isopropanol, ethyl acetate and n-hexane in the mixed solution is 5: 3.8-4.2: 4.8-5.2.
10. Use of the fullerol/palladium nanocomposite photocatalyst of claim 1 on CO2And (4) carrying out photocatalytic reduction.
CN202111075752.0A 2021-09-14 2021-09-14 Fullerol/palladium nano composite photocatalyst and preparation method and application thereof Pending CN113926487A (en)

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